Preparation of synthetic ammonia.



, v'oirs "of nitrids.

"nnrrnn srAT s IHSLTEN T,(1) TI'1'7FI(-'JE i canm'ron ELLIS, or mon'rcram,

No Drawing.'

To all whom it mag concern:

Be it known that I,- Cannn'ron Ennis, a citizen of the United States, and a resident of Montclair, in the county of Essex and State of New Jersey, have invented certain new and useful Improvements. in the Preparation of Synthetic Ammonia,of which the following isa specification.

This application-relates to the synthetic formation of ammonia by contacting a mixture of hydrogen and nitrogen with certain catalytic material and relates especlally to the use of carbids and othen similar compounds as catalytic agents, in connectlon with said process.

I In carrying out the invention in one preferred form, a mixture of nitrogen and hyclroge'n, well purified and particularly being free from oxygen ort oxldizing agents, is passed over catalyticmat'erial of the character indicated and maintained at a temperature of 40 O600 C. and held under a pressure ordinarily substantially below 100 atmospheres and preferably above 30 or 40 atmospheres and in particular for the catalyzer specifically hereinafter referred to,

held between about'60-80 atmospheres, as

,within these limits a. particularly satisfac tory degree of hydridation and conversion is secured under effective condltions of operation, which render such critical pressures beneficial. A

The mixture of hydrogen and nitrogen preferably should be in the proportion of 3: 1 and as stated should be free from oxy-.

gen and also from catalyzer'poisons such as s'ulfur'and the like. In place of passing the mixture of the gases over the catalyzer the gases may be separatel .passed'in alternation. Under these conditions less desirable results usually are obtained because of the complication in apparatus and the neces- .sityof having fair large containers under high pressure in w 'ch the catalytic material iscontained, toserve as storage reser- In the preferred form of the invention, thematerial dfia catalytic nature is placed in aftribbf considerable length with respect to-dia'meter, andis packed thereinin such a manner that the gases pass through the catalyticjbd in a positive manner, so that an ef- -.fective exposure of. the catal tic surface is obtained without retardation ue to slowness of diffusion as may easily occur in treatmg NEW JERSEY, nssrenon BYE, new You;

Specification of Letters Patent.

poses, whose nitrogen-occludin 'r-o cLIN'roN shurkms, or

PREPARATION or sYn'rnErro Ammonia.

gases over the upper surface of such mass.

Patented July 23,1918. Application a May 31, 1916. Serial 1%; 100,835.

' The particular jcatalytic material employed herein is a carbid, especially the carbids of cobalt, nickel, copper, iron, palladium, ;platinuin, chromium, manganese,

titanium, molybdenum, vanadium, thorium, a zirconium, etc., andstill more particularly the carbids of cobalt, nickel, iron and maliganese, which metals aflord carbids. that are well' adapted for treatment with the mixed hydrogen and nitrogen gases as distinct from the alternate method of gas treatment, reactin to a greater or less degree to give f nitri s or carbo-nitrids' or similar bodies during the course of the reaction.

Illustratively, a catalyzer may be prepared by heating a mixture of e uivale'nt propor- -tions of nickel and coba t hydrate. with charcoal under reducing conditions producing a greater or lessquantity of a carb'id of the metal preferably in a finely-divided and porous state, which is eculiarly suited for the present purposes. referably an excess of charcoal vover that required to form-more or less of the carbid is caused to be present and serves as an hydrogen-occluding agent,

which condition is useful in carrying out the present invention. A, mixture of one part of nickel-cobalt hydrate or of iron-manganese hydrate, with two parts of charcoal heated in a reducing furnace to about 600 C. or higher, if necessary, furnishes a catalytic agent well adapted for the pi s'ent pur- I properties may be enhanced by the additlon 0B vanadium, titanium, manganese, cerium and the like, using for example three parts of nickel carbid, and two parts of charcoal with one part of any of the metals mentioned.

The catalytic agent derived in this manner or in any other suitable wa is usually prepared under conditions such that it may be exposed to the hydrogen andnitrogen gas mixture without any undue oxidation, and the gas mixture is allowed to passfover or preferably .therethrough under the pressure and'temperature indicated. A tubular container enables a suitable layer'of .the porous mass to be penetrated by the gas. If the catalytic agent iSfsoEprepared to produce granular particles,ra; porous mass is obf lar fragments does not greatly hinder the gas flow, yetall parts of the catalyzer are bathed with gas of practically uniform quah ity and instead of restricted local action a. 6 reaction throughout the catalytic material is better obtained.

Garb-M oi cerium may be employed alone or in conjunction with the'foregoing. A mixture of one part of cerium carbid and two parts of carbon may be used..

The combination or association of av metal and a metalloidal element to form a catalyst for use at pressures under .100 atmospheres,

preferably 60-80 atmospheres, is particularly desirable when using the catalyzer as hydrogen and nitrogen through a catalytic agent comprising nickel-cobalt carbid.

2. The process of making synthetic ammonia which comprises bringing a mixture of hydrogen and nitrogen into-contact with a catalytic agent comprising nickel-cobalt T carbritl and free carbon.

GARLETON' ELLIS. 

